Combustion Nitrogen Analyzers

elementar Americas, Inc.

SERA-IEG Annual Meeting

June 21, 2009

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CombustionCombustion Nitrogen AnalyzersNitrogen AnalyzersAgendaAgenda

elementar Americas Inc.history and current organization

elementar product line

applications overview

Analyzer technology and operationChemistry / Process flow / Mechanical design

Selecting an instrumentdesign considerations

choices - Rapid N cube / vario MACRO cube / vario MAX

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elementar historyTechnology Development

1868 - high temperature techniques developed in Hanau, Germany

1878 - Dennstedt Patent

1925 - Nobel prize for CHN analysis

1990 - first Macro scale elemental analyzer

1999 - first MAX analyzer

2006 - first cube platform analyzer introduced

Organization1868 - Heraeus

1993 - management buyout forms elementar GmbH

1999 - elementar Americas Inc formed 2008 - Isoprime Ltd acquired (Isotope Ratio Mass Spectrometers)

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elementar Organization

Manufacturing, R&D and applications labs elementar Analysensysteme GmbH

CHNS/O Elemental Analyzers

Located in Hanau, Germany (30 minutes from Frankfurt Airport)

Isoprime LtdWholly owned subsidiary

Isotope Ratio Mass Spectrometers

Located near Manchester, U.K

Sales, service, applications, and supplies elementar Americas, Inc.

Responsible for sales and service in USA, Canada, Mexico and Central America

based in Mt. Laurel, NJ (30 minutes from Philadelphia)

Service from NJ, IN, CO, Toronto

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elementarElemental Analyzer Product Line

Micro scale CHNS/Ovario MICRO cube

vario EL cube

Macro scale CHNS/Ovario MACRO cube

vario MAX

rapid N cube & rapid CS cube

TOCliquiTOC

vario TOC cube

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vario MAX vario MAX CN CN

Macro N/CN Elemental Analyzers

rapid N rapid N cubecube

vario vario MACRO CN MACRO CN

cubecube

Elemental Analyzer Technology and Operation

Core OperationsCombustion

Gas separation

Gas detection

Chemistry

Process Flow Diagram

Other operationsSample preparation

Autosampler and sample feeding

Software

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Elemental AnalyzerCore Operations

CombustionSample combusts in furnace at 950 deg C to 1200 deg C Sample drops into crucible or is lowered into center of combustion tubeJet injection of oxygen via lance right over/at sample

Creates turbulent flow around samplelike blowing on a fire

Three tube low voltage furnace with 10 year warranty

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Elemental AnalyzerCore Operations

Gas SeparationHelium or CO2 carrier gas pushes combustion gases through analyzer.

C, H and S combustion gases are trapped in separate columns, then sequentially released (aka “purge and trap”).

N2 gas is not trapped. It flows straight thru columns.

Gas DetectionTCD – Thermal Conductivity DetectorUtilizes a Wheatstone bridge circuit to compare relative thermal conductivity differences between the carrier gas and analyte gasCritical system componentElementar own designLarger dynamic rangeVery special thermistors which are not harmed by high oxygen content.Allows for suspension of carrier gas flow without any harm, even at operation temperature.

Elemental AnalyzerElemental AnalyzerCore OperationsCore Operations

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Elemental AnalyzerChemistry

CombustionR-N + O2 ----> N2 + NOx + O2 + CO + CO2 + CH4 + X- + SOx + H2O

Post CombustionCO + CH4 ---CuO & Pt --> CO2 + H2O

ReductionNOx+O2 +SO2--tungsten--> N2+WO3 +CO (trace)

CO + CuO --------> CO2

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Elemental AnalyzerMore Chemistry

Removal of other gasesX- via reaction with silver wool

H2O via condensation, membrane dryer and Sicapent

trace S02 via reaction with tungsten

Nitrogendetected by TCD

Carbon Dioxiderapid N – “fades” into carrier gas

vario MAX and vario MACRO – separated on purge and trap column, then released and detected by TCD.

N2

CO2

CO + CH4 ---CuO & Pt --> CO2 + H2O

R-N + O2 ----> CO + CO2 + CH4 + N2 + NOx + SOx+ H2O + X- + O2

sample

COCH4

XX X

NOx

H2O

X

N2

SO2

X X

X-

X

CO2

O2

NOx + CH4+O2 +SO2--tungsten--> N2+WO3 +CO (trace)

WO3

CO2

CO2

N= 2.00%C= 3.00%

Oxidation

Post Oxidation

Reduction

Process Flow Diagram and Chemistry

Gripper Arm lowers crucible containing sample into combustion tubeOxygen is injected over sampleSample combusts

Combustion gasses are producedWe are interested in N2 and CO2.Other gases must be converted or removed.

Methane and carbon dioxide are oxidized in post combustion tube.Carbon dioxide flows through instrument and is trapped in column

Halogens are removed by reaction with silver wool in post combustion tube.

Water is removed by a three stage dryer:condensationmembrane dryerSicapent

Reduction TubeExcess oxygen reacts with Tungsten.SO2 is adsorbed by tungsten.

O2

Reduction Tube:Oxides of nitrogen reduce to nitrogen gas.Nitrogen flows to TCD. Computer integrates peak and calculates N2 percent.

CO2 column is heated.CO2 flows to TCD. Computer integrates peak and calculates CO2 percent.

Ash

Ash

Gripper arm removes crucible with ash from combustion tube.Crucible deposited in recepticle for re-use

Process Flow Diagram Comparison

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Replace robotic arm with Carousel

and ball valve

vario MACRO cube CN

Replace robotic arm with Carousel

and ball valve

Rapid N cube

CO2

Remove CO2 adsorber

Add CF Hybrid

Elemental Analyzer Technology and Operation

Core OperationsCombustion

Gas separation

Gas detection

Chemistry

Process Flow Diagram

Other operationsSample preparation

Autosampler and sample feeding

Software

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Sample Preparationrapid N cube and vario MACRO cube

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60 position open carousel - add samples at any time during run - optional 80 or 120 position carousel

Variety of foils/capsules

Sample Pressing Tool

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rapid N cube and vario MACRO cube have slightly different designs.

Both designs provide: inherent blank-free system

reliable function

keeps air out of the system

very long lasting operation

easy maintenance

Ball Valve Sample Feedrapid N cube and vario MACRO cube

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rapid N Sample IntroductionBall valve with nickle flap flange

Straight-through Ball Valve actuates.

Sample falls to top of nickel flap flange.

Nickel flap flange actuates magnetically.

vario MACRO cubepatented zero-blank ball valve

Position 1; Sample falls into ball valve cavity.

Position 2; Ball valve cavity purged with helium.

Position 3; Ball valve opens to combustion tube.

Position #1 Position #2 Position #3

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vario Max Sample preparation

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vario MAXsample feeding

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vario MaxSample Feeding

Robotic “gripper arm”Lifts reusable crucible from carousel.

Lowers crucible into the combustion tube (~1000 C)

Lifts to removes crucible and ash

Deposits the ash & crucible in catch bin

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Analyzer Software

intuitive interface

easy editing

view graph during analysis

great export functionality

21CFR part11/LIMS/GLP conformity

Elemental Analyzer Technology and Operation

Core OperationsCombustion

Gas separation

Gas detection

Chemistry

Process Flow Diagram

Other operationsSample preparation

Autosampler and sample feeding

Software

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1000

 

300

Sample   

Size 200

(mg Organic  

Content) 50

 

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C S N CN CNS CHNS CHN O Cl

Operating Mode

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Macro sample N/CN Analyzer Selection maximum capacity (organic) and

capability

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Vario MAXBest choice for CN or N samples that are non-homogeneous, very low in concentration, wet , high ash or difficult to handle.

Vario MACRO cubeOptimum economics for larger CN samples with easier handling characteristics (dry, semi-homogeneous).

Capital cost lower than MAX

CF Hybrid technology optimizes consumables cost

Rapid N cubeOptimum economics for larger N samples with easier handling characteristics.

Capital cost lower than MACRO

CO2 carrier gas reduces gas cost

Macro sample N/CN Analyzer Selectionrecommendations

vario MACRO cubeElementar´s answer to YOUR

analytical needs

The new cost-effective macro analyzer family for

N/CN for protein, plant material or soil analysis

CNS CHNS for plant and soil,

environmental or oil samples

CHN for the analysis of coal, biomass or combustible solid waste

Options:

„Standard options:“

- Capsule press for liquids

- Pressing tool

IR Detectors for special applications:

- low level sulfur analysis

- low level oxygen analysis

- chlorine analysis

VLS, vario liquid sampler

Continuous flow Hybrid (CN only)

Options:Automatic liquid injector for the „cube“

family liquid sample feeder for 60 samples, plus flushing and waste positions

easy setup, replaces standard ball valve and carousel

can be used on: vario EL cube vario MICRO cube vario MACRO cube

Launched in 2008, first installations successful

CF-Hybrid technique for CN mode

The newly developed hybrid technology serves for longer lifetime of consumables.

Only a fraction (approx 50%, adjustable) of the combustion gas is lead through the reduction tube in continuous flow mode, saving valuable reduction metal and expansion of uninterrupted operation time.

Features:

Easy to install and remove (1-2 minutes!), so the user can choose between highest sensitivity or highest throughput.

Active flow control.

Ideal for high-throughput laboratories with similar sample matrix.

Elementar thanks you for your attention !

For further information please contact us under:

Web Page: www.CHNOS.com

e-mail: info@elementar-inc.com